高演化烃源岩岩石热解和总有机碳标准物质研制  

Preparation of certified reference materials for rock-eval and total organic carbon of postmature source rock

作　　者：杨佳佳[1] 孙玮琳[1] 徐学敏[1] 秦婧[1] 沈斌 张小涛 栗敏 汪双清[1] YANG Jiajia;SUN Weilin;XU Xuemin;QIN Jing;SHEN Bin;ZHANG Xiaotao;LI Min;WANG Shuangqing(National Research Center for Geoanalys,Beijing,100037)

机构地区：[1]国家地质实验测试中心,北京100037

出　　处：《地质学报》2020年第11期3515-3522,共8页Acta Geologica Sinica

基　　金：中国地质调查局地质调查项目(编号DD20190086);国家自然基金青年基金项目(编号41702159)资助的成果。

摘　　要：南方下古生界海相页岩是我国页岩气勘探开发的重点地层,普遍具有时代老,热演化程度高的地质特征。已有基于常规测试条件制备的岩石热解及总有机碳分析标准物质无法满足此类高演化样品分析的需求,一定程度上制约了页岩气勘探开发进度。研究采集贵州织金龙潭组的泥岩及煤样,按照国家一级标准物质研制标准和规范,研制2件高演化烃源岩标准物质(编号为GBW07499和GBW07500),定值指标S2、Tmax和TOC。经均匀性检验,三个指标的F值均小于临界值F(0.05)(v1,v2),样品单元间均无显著性差异,均匀性良好。经两年时间考察室温条件下特性量值S2、T(max)和TOC的变化趋势,结果表明拟合直线斜率|b1|<t0.05,S(b1),稳定性良好。经多家权威实验室联合定值,全部定值分析数据符合正态和近似正态分布,且等精度,给出认定值和不确定度分别为:S2为1.09±0.10mg/g,T(max)为633±3℃,TOC为26.8%±1.3%;S2为6.31±0.48mg/g,Tmax为613±4℃,TOC为63.1%±3.4%。2件标准物质可满足高演化样品岩石热解和总有机碳分析测试工作的需求,为解决该类样品分析过程中仪器校准、方法评价和数据质量监控等问题提供物质基础,有效提升测试数据质量。Marine shale in the lower Paleozoic is generally characterized by old age and high thermal evolution,which is the key stratum for exploration and development of shale gas in south China.At present,the reference materials(CRMs)of rock-eval and total organic carbon(TOC)analysis based on conventional conditions are difficult to meet the analysis of high thermal evolution samples,which severely restricts the progress of exploration and development of shale gas.For this study,mudstone and coal samples in the Longtan Formation are collected from Zhijin city in Guizhou.According to national primary reference materials specifications,two postmature sourcerock CRMs(GBW07499-GBW07500)have been developed,which give the certified values of S2,Tmax and TOC.For the homogeneity test,the calculated F values in 2 rock-eval and total organic carbon CRMs obtained by analysis of variance(ANOVA)were less than the critical F values at the 95%confidence level,indicating no obvious differences between units and within units.The results showed that 2 CRMs had good homogeneity.The calculated test statistic b1 of 2 CRMs during the 24-month observation period was statistically insignificant,indicating that 2 CRMs were stable.All the datas that 9 qualified laboratories were selected to give are in accordance with normal and approximate normal distribution and also equal accuracy.The standard materials provided certified values of S2,Tmax and TOC with uncertainties:S2=1.09±0.10 mg/g,Tmax=633±3℃,TOC=26.8%±1.3%,S2=6.31±0.48 mg/g,Tmax=613±4℃,TOC=63.1%±3.4%.The CRMs can provide material basis for solving the problems of instrument calibration,method evaluation and data quality monitoring in the process of rock-eval and total organic carbon analysis,which effectively improve the quality of test datas.

关 键 词：标准物质 岩石热解 总有机碳 高演化 

分 类 号：P618.13[天文地球—矿床学]